Method of making combination stain fillers using dye concentrates



Patented June 1, 1954 UNITED STATES PATENT OFFICE METHOD o'F MAKINGCOMBINATION s'rAIN FILLERS USING DYE coNcENfrRATEs Herman Nack, Troy,and George L. Denist'on,

Dayton, Ohio, assignors to Chadeloid Corporation, Dayton, Ohio, acorporation of Delaware Application March 12, 1951, Serial No. 215,168

2 claims. (c1. 26o-33.2)

This invention relates to improvements in stain filler compositions.More particularly the invention relates to a new method of producing acomposition of the permanent staining type.

Stains and stain fillers of the so-called permanent type are now wellknown in the art. These compositions are characterized by nonfading andnon-bleeding properties and by the important feature of penetration ofthe wood surface to which they are applied Without undesirable raisingof the grain. These compositions are produced by solving aniline dyestogether with binder resins, inert fillers, wetting agents, dispersingagents and thinning mixtures in suitable solvents.

The present invention contemplates the provision of a method for themaking of a stain filler composition which will have increased powers ofpenetration of the wood and increased coloring ability.

The invention further contemplates ka stain filler of the glycol ethertype having particular proportions of at least two glycol ethers in thesolvent for the dye.

The attainment of the objectives of the invention is procured by makinga solution of a dye concentrate in a glycol ether solvent containing amixture of at least two ethers and thereafter combining the solved dyewith a neutral paste containing the inert filler, the resin binder,wetting agents, dispersing agents and thinners.

It has been found that the dye solvent for acid organic dyestuifpreferably contains diethylene glycol monomethyl ether to the extent ofbetween about 12 to 20 parts, the balance being ethylene glycolmonomethyl ether. A particularly Isatisfactory solvent material consistsof 16.2 parts diethylene glycol "monomethyl ether and 83.8 partsethylene glycol monomethyl ether by weight.

It has also been found that the most desirable stain-filler is obtainedif approximately 14 parts of a dye concentrate made up as set forthabove are combined with approximately V86 parts of a neutral fillerpaste. While other ratios of these components may be utilized toadvantage the above ratio yields particularly effective results both asto covering power and the penetration of the wood. A

It is believed that when the'particlar Sequence of combining steps 'isfollowed as setforth above the dyestuff enters into solution morethoroughly and is retained in solution upon the addition 'of the fillerpaste composition. Thus preferential absorption of the dye by thefillers and binder materials is avoided, resulting in an improvedstaining action of the stain-filler composition. Thus the improvedfiller yields increased coloring 2 power as well as increasedpenetration of the wood fibers. y

The components comprising the neutral paste filler are resins, wettingagents, dispersing agents, inert fillers and thinning agents.

Binder resins which are particularly suitable are the phenolic aldehyderesins, urea-formaldehyde resins, esteriiied resins or frosins, andresins of the alkyd type such as the polyesters of phthalic acid andethylene glycol.

Wetting agents which are particularly suitable are 'morpholi'ne which isa secondary amine, sulfonates and sulfates such as the sodium salt ofalkyl naphthalene sulfonic acid (Darvan) and sodium heptadecyl sulfate(Tergitol #7) have been found to be most satisfactory. Y

Dispersing agents for th'e filler may be selected from suchrepresentative groups as the polyvinyl family, metal soaps and esters.Pclyvinyl alcohol is preferred because it 'acts as a thickening agentfor the stain composition as well as acting as a disperser. Thiscompound may be used in proportions of 5 vto v30 parts by weight ofsolution.

Thinners commonly used in this vtype of cornpound and suitable for thepractice of this invention are methanol, tolu'ol, benzene, or mixturesthereof.

The inert fillers may be Silenc, which is a hydrated precipitatedcalcium silicate; Silex, which is a silica; diatomar'ze'ous earth;asbestine, clay, and similar materials'. Inert Apigments such as burntumber, activated carbon, iron oxides, may also be used.

The dye'stuifs found to be r.particularly useful in the practice of thepresent invention are acid organic mater-ials ofthe -aniline type*characterized by fastness to light and ready solubility in vehicles ofthe hydroxyl group. Thus, for example, the following dyestuifs may beused alone vor in combinations to produce -'ali'ncst any desiredstaining color: Buffalo Black NBR Conc. 126%, Black Stain B34951,Nigrosine 4523J Conc. Powder.; the following yellow Adyestuifs: FastWool Yellow 3 GL Conc. 125%, Fast Light Yellow 3G EX. Conc., Fast vLightYellow DSGA; the fol-l lowing orange-yellow dyestuffs: Metanil Yellow1955, Calcocid Yellow MXXX Conc.; the lfollowing orange dyestuffs: FastLightOran'ge 2G, Fast Light Orange GA Conc.; the following reddyestuffs: izo rRubine Ex. Conc. 133%, Calcocid Milling-Red 7B Conc.,Camoisine BA Extra Conc. CF, Chromolan -Bordeauz R. Croceine ScarletMoo.

The particular relative proportions of these components comprisingsuitable neutral filler pastes for the `pi'a'ctice 'of the invention areWell kho'wnto the fart'andform'no part lof the present invention, theonly requirement being compati- Example I A dye concentrate solution wasfirst made utilizing the following materials in parts by weight:

6 parts red mahogany dye 50 parts of a solvent containing:

80 Darts ethylene glycol monomethy1 ether 20 parts diethylene glycolmonomethyl ether The dye will be completely solved in the solventmaterial. Thereafter a neutral paste was made up cone sisting in partsby weight of 40 parts of an alkyd type resin having a phthalic anhydridebase 15 parts polyvinyl alcohol l parts morpholine 20 parts hydratedprecipitated calcium silicate This neutral paste was then combined withthe dye solution in the fol-lowing proportions in parts by weight:

14 parts dye solution 86 parts neutral filler The stain-lier thus formedwhen applied to Wood surfaces penetrates the pores and colors the woodexceedingly Well.

Example II The following dye concentrate solution was made utilizing inparts by Weight:

4 parts croceine orange 2 parts scarlet red moo 3.4 parts Buffalo black5G parts of a solvent containing:

16.2 parts diethylene glycol monomethyl ether 80.3 parts ethylene glycolmonomethyl ether The dyes were completely solved in the glycol ethers.

A neutral filler paste was then made up containing in parts by weight:

30 parts phthalic anhydride base alkyd resin parts polyvinyl alcohol 10parts aluminum stearate 5 parts morpholine 30 parts hydratedprecipitated calcium silicate 10` parts toluol parts methanol rlhis dyesolution and neutral filler paste were then combined in the followingproportions in parts by weight:

14 parts dye solution 86 parts neutral filler This stain-filler whenapplied to a wood surface colored the same very weil and was a decidedimprovement over the same composition formed by mixing all thecomponents in one operation.

Example III The following dye concentrate solution was made utilizingthe following materials in parts by Weight:

2.4 parts mahogany dye 2l) parts of a solvent containing:

8G parts ethylene glycol monomethyl ether 28 parts diethylene glycolmonomethyl ether The dye was completely solved in the solvent material.

Thereafter a neutral filler paste was made up consisting in parts byweight of 10.0 parts methanol 10.0 phthalic anhydride glycerol resin(Beckosol 3.0 parts polyvinyl alcohol 40.0 parts toluol 60.8 parts SilexThis neutral paste Was combined with a dye concentrate solution in thefollowing proportions in parts by weight:

20 parts dye concentrate solution 8O parts neutral filler It will beunderstood that while there have been given herein certain specificexamples of the practice of this invention, it is not intended therebyto have this invention limited to or circuinscribed by the speciiicdetails of materials, proportions or conditions herein specified, inView of the tact that this invention may be modied according toindividual preference or conditions without necessarily departing fromthe spirit of this disclosure and the scope of the appended claims.

We claim:

1. A process for the production of wood stain fillers having enhancedpenetration and coloring characteristics comprising the steps of firstforining a solution of red mahogany dye in a mixture of parts ofethylene glycol monomethyl ether and 2O parts of diethylene glycolmonornethyl ether, secondly forming a neutral paste containing an alkydresin comprising the reaction product of phthalic acid and ethyleneglycol, a filler, a dispersing agent and a wetting agent, and thereaftercombining the dye solution with the neutral iiller .paste to produce thesaid stain filler.

2. A process for the production of wood stain llers having enhancedpenetration and coloring characteristics which comprises the steps offorming a dye concentrate comprising dissolving lan acid organic dye ina mixture of diethylene glycol monomethyl ether and ethylene glycolmonomethyl ether, wherein ethylene glycol monomethyl ether is present inthe greater proportionate amount, said mixture of glycol etherscontaining in 1GO parts by weight between about `.l2 to 20 partsdiethylene glycol monomethyl ether and the balance being ethylene glycolmonomethyl ether, providing a paste comprising inert filler and a resinselected from the group consisting of phenol formaldehyde resin, ureaformaldehyde resin, and polyesters of phthalic acid land ethyleneglycol, and mixing said paste filler with said dye concentrate toproduce a combined stain and iller.

References Cited in the le of this patent UNITED STATES PATENTS NumberName Date 2,161,503 Bush June 6, 1939 2,338,149 Walker et al Jan. 4,1944 OTHER REFERENCES Elvanol, Polyvinyl Alcohols, by the Du Pont Co.,published 1947, pages 7 and 20.

2. A PROCESS FOR THE PRODUCTION OF WOOD STAIN FILLERS HAVING ENHANCEDPENETRATION AND COLORING CHARACTERISTICS WHICH COMPRISES THE STEPS OFFORMING A DYE CONCENTRATE COMPRISING DISSOLVING AN ACID ORGANIC DYE IN AMIXTURE OF DIETHYLENE GLYCOL MONOMETHYL ETHER AND ETHYLENE GLYCOLMONOMETHYL ETHER, WHEREIN ETHYLENE GLYCOL MONOMETHYL ETHER IS PRESENT INTHE GREATER PROPORTIONATE AMOUNT, SAID MIXTURE OF GLYCOL ETHERSCONTAINING IN 100 PARTS BY WEIGHT BETWEEN ABOUT 12 TO 20 PARTSDIETHYLENE GLYCOL MONOMETHYL ETHER AND THE BALANCE BEING ETHYLENE GLYCOLMONOMETHYL ETHER, PROVIDING A PASTE COMPRISING INERT FILLER AND A RESINSELECTED FROM THE GROUP CON-